Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | (2RS,3RS)-2-(2,4-difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol | HCID 9882302 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 9829484 | HCID 9829484 | 50.2% |
Reaction Steps
To dichloromethane (20 ml) was added (2RS,3RS)-2(2,4-difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol (0.3 g). To the mixture was added dropwise at room temperature a dichloromethane solution (10 ml) of iodine (0.17 g). The mixture was stirred for 30 minutes at room temperature, washed with a 5% aqueous solution of sodium hydrogensulfite and dried (Na2SO4). The solvent was then distilled off under reduced pressure. The residue was subjected to a silica gel chromatography (2.5×30 cm), eluting with ethyl acetate - hexane (4:1). The objective fraction was concentrated. Addition of diethyl ether-hexane (2:1) to the concentrate gave bis[3-(2,4- difluorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)-2butyl] disulfide (Compound 15, 0.15 g) as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05177094 |
|---|
| Source dataset | uspto-grants-1993_01 |
|---|
| ORD ID | ord-94ab966cd84b4040957360da39e252cf |
|---|
| Source note | uspto-grants-1993_01 |
|---|